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晶棒法

图示为一晶棒法所用仪器。仪器主体由石英制作(1)接真空泵抽真空(2)6 mm 钼电极,(3)钼网,(4)原料金属置放处,(5)钨丝

晶棒法,又称为碘化物精炼法,或以开发者为名的范·亚克-德·波耳制程,是1925年两位荷兰化学家安东·范·亚克英语Anton Eduard van Arkel以及扬·德·波耳英语Jan Hendrik de Boer所开发的金属精炼方法。[1] 晶棒法是最早能够商业化制造高纯度延性的工业制程。晶棒法也可以小量生产超高纯度的钛(或锆)。晶棒法的概念牵涉到用气相去跟低纯度的金属作反应产生气相碘化物,碘化物飘向加热灯丝后受热分解出高纯度的金属。晶棒法今已多被克罗尔法取代。

制程

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如下图所示,低纯度(这里主要探讨钛跟锆)在外接真空泵的容器中通卤素加热至50–250 °C,四碘化钛(TiI4)、四碘化锆(ZrI4)等等中间产物就会开始出现并挥发,把杂质留在原处。利用物质在低压下沸点降低的原理(常压下四碘化钛熔点150 °C、沸点377 °C,四碘化锆熔点499 °C、沸点600 °C),挥发的气相碘化物飘到1400 °C的白炽灯丝(钨丝)上受热分解。 随着越来越多纯金属积附在灯丝上,灯丝的电阻会下降,以至于必须通更大的电流或时时收集产物才能维持灯丝的发热功率。整个制程视设备情况,可历时短至数小时,长至数周不等。

总体而言,晶棒法视对不同金属之反应性决定要在制程中添加的卤素或卤素比例,俾利整个输送机制进行。只有钛、锆、铪这三种金属曾经用晶棒法进行工业规模生产,今之晶棒法可谓没落,仅用于特殊纯度需求的小量生产。[来源请求]

晶棒法示意图,字母M 指称金属,图下方的M是低纯度金属,附着在图上方钨丝上的M是高纯度金属

图库

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陈列数种晶棒法提炼的金属:

参考文献

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  1. ^ van Arkel, A. E.; de Boer, J. H. Darstellung von reinem Titanium-, Zirkonium-, Hafnium- und Thoriummetall. Zeitschrift für anorganische und allgemeine Chemie. 1925, 148 (1): 345–350. doi:10.1002/zaac.19251480133 (德语). 
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晶棒法
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